This invention relates to methods for intercalating chalcogenides. In the past, chalcogenides have been intercalated under conditions such that the quantities of the reactants must be controlled and generally past methods of preparation required elevated temperatures and significant periods of time (ranging from several hours to several months) for preparation. In contrast thereto, the present methods of intercalation permit the degree of intercalation to be controlled very readily by controlling the current passed into the system without the need to control the quantities of the reactants. Furthermore, the present methods of intercalation permit control and monitoring of the thermodynamic activity of the intercalated specie as well as permitting the reaction to be performed quite rapidly at room temperature, thus eliminating the problem of intercalating those chalcogenides which might otherwise be decomposed at elevated temperatures. The resultant intercalated compounds are known to be useful as lubricants, X-ray diffraction grating crystals, superconductors, and thermo-electric elements, e.g., see published German patent application 2,061,162 , Australian Journal of Chemistry, Volume II, page 471 et seq (1958) and the Journal of Chemical Physics, Volume 58, page 697 et seq (1973).